MIL-DTL-14067C
4.5.3 Volatile material at 105oC. Approximately 5 grams of the sample shall be weighed
into a tared dish and heated in an oven for 3 hours at 105oC. Remove from oven and place into a
dessicator to cool. Reweigh sample and the loss in weight shall be calculated as percent volatile
material at 105oC.
Percent volatiles =
Where:
A = loss in weight, gm.
B = weight of sample, gm.
4.5.4 Carbides.
4.5.4.1 Gas chromatography with flame ionization detection (GC/FID).
4.5.4.1.1 Overview. The following procedure is used to determine the amount of
magnesium carbide (acetylide) in magnesium. Sample is dissolved in 5 % sulfuric acid and
acetylene thus produced is measured by GC/FID. The method can be extended to measure other
types of carbides present provided that appropriate standards are available and the instrument
method is modified appropriately.
4.5.4.1.2 Reagents.
a. Sulfuric acid (H2SO4), concentrated 95 98 % wt, ACS reagent grade.
b. Distilled water.
c. Sulfuric acid, 5 % wt aqueous solution, made by dissolving 30 milliliters of concentrated
sulfuric acid in enough distilled water to make 1000 milliliters of solution. Scale the
amounts proportionally to make more or less reagent depending on the number or
samples to be run. Quantity: 100 milliliters per sample and 50 milliliters per standard.
4.5.4.1.3 Gas standard.
a. Compressed gas cylinder containing 1 mole % each C1-C2 hydrocarbons, i.e. methane,
acetylene, ethylene, and ethane, e.g. Sigma 23462 or equivalent.
b. Matching regulator required; see supplies and equipment (4.5.4.1.4).
4.5.4.1.4 Supplies and equipment.
a. GC column: Agilent J&W CarbonPLOT 60 m/0.32 mm/1.5micometers
(length/diameter/film thickness) or equivalent capable of resolving C1-C2 hydrocarbons
in less than 10 minutes. Quantity: 1.
b. Round-bottom-3-neck flask, 500 milliliter, 24/40 ground-glass ports, e.g. Kontes 606000-
1024 or eq. Quantity: 1.
c. 24/40 ground-glass barbed adapter, e.g. Kontes 182900-2440 or eq. Quantity: 2.
d. Addition funnel with stopcock, >50 milliliter, 24/40 ground glass joint, e.g. Ace Glass
7257-50 or eq. Quantity: 1.
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